CN115477832B - Preparation method of PBAT degradable mulching film - Google Patents
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Abstract
A preparation method of a PBAT degradable mulch film comprises the following raw materials: the invention relates to a degradable mulching film, which is prepared from PBAT, a light stabilizer, an antioxidant, polylactic acid, modified attapulgite, acetyl triethyl citrate, a styrene-maleic anhydride copolymer, a compatilizer and a lubricant by taking the PBAT and the polylactic acid as the bases and adding the modified attapulgite, the styrene-maleic anhydride copolymer and other auxiliary agents to obtain the degradable mulching film with good light weight and toughness, and further improves the tearing strength of the degradable mulching film.
Description
Technical Field
The invention belongs to the field of degradable mulching film preparation, and particularly relates to a preparation method of a PBAT degradable mulching film.
Background
In the beginning of the 50 s, the plastic film mulching cultivation technology is first popularized in japan, and the plastic film mulching cultivation technology is introduced from japan in 1978 in China, so that the yield of crops is greatly improved, and particularly in recent years, the successful popularization and application of the drip irrigation technology under the film further promotes the leap development of the plastic film mulching technology. Because the mulching film has the functions of heat preservation and moisture preservation, white pollution caused by flooding disaster is avoided while the yield and income are increased; after the agricultural mulching film is abandoned, a treatment mode of picking up and burning or turning over the agricultural mulching film to cover the agricultural mulching film is generally adopted, and the non-degradable film is accumulated along with the growth of the year and month to be far beyond the bearing capacity of soil.
The degradable agricultural mulching film has good biodegradability and the performance of heat preservation, moisture preservation and soil moisture preservation required by plants, and can replace the traditional PE mulching film; at present, the performance of the degradable agricultural mulching film is lower than that of a PE film under the same condition, wherein the performance of the degradable agricultural mulching film is most obvious in terms of tearing strength; the improvement of the service performance is achieved at the expense of cost, such as thickness increase, raw material use with higher price and more complex processing technology, so that the degradable mulching film is difficult to popularize and apply on a large scale. Therefore, how to improve the tearing strength of the full-biodegradable mulch and reduce the cost is a key point for solving the popularization and use problems of the degradable agricultural mulch.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a PBAT degradable mulch film.
The invention adopts the following technical scheme:
the preparation method of the PBAT degradable mulch film comprises the following raw materials in parts by weight: 50-70 parts of PBAT, 0.8-2 parts of light stabilizer, 0.7-1.5 parts of antioxidant, 25-35 parts of polylactic acid, 10-15 parts of modified attapulgite, 0.1-0.5 part of acetyl triethyl citrate, 3-5 parts of styrene-maleic anhydride copolymer, 1-2 parts of compatilizer and 0.5-0.8 part of lubricant;
the preparation method comprises the following steps:
step one, weighing and mixing PBAT, polylactic acid and modified attapulgite according to the required weight parts, and then heating and baking at 80-100 ℃ until the water content is lower than 0.5%;
step two, weighing other raw materials according to the required weight parts, and then sending the mixture obtained in the step one into a high-speed mixer, and uniformly mixing to obtain a premix;
step three, putting the premix obtained in the step two into a double-screw extruder, and controlling the extrusion temperature between 150 and 180 ℃ to obtain film blowing master batch;
and fourthly, blowing the film blowing master batch into a film by a film blowing machine to obtain the PBAT degradable mulch film.
Preferably, the preparation method of the modified attapulgite comprises the following steps:
(1) Crushing attapulgite to 10-20 meshes, adding the crushed attapulgite into water, uniformly stirring, soaking for more than 12 hours, centrifuging, filtering, and drying for later use;
(2) Adding the attapulgite treated in the step (1) into a phosphoric acid solution, stirring and heating, wherein the stirring speed is 180-250r/min, and the heating temperature is 80-90 ℃; then filtering to remove phosphoric acid solution, washing attapulgite with weak base solution to neutrality, washing with deionized water for 2-3 times, and drying for standby;
(3) Raising the temperature of the attapulgite obtained in the step (2) to 250-300 ℃ from room temperature, enabling water vapor to contact and react with the attapulgite through inert gas, starting to cool after the reaction is finished, and stopping adding the water vapor; and after the temperature is reduced to room temperature, taking out the attapulgite, washing and drying until the water content is lower than 5%, and grinding and crushing to obtain the nano-grade modified attapulgite.
Preferably, in step (2), the mass concentration of the phosphoric acid solution is 5%.
Preferably, the lubricant is polyethylene wax or oleamide.
Preferably, the light stabilizer is epoxidized soybean oil.
Preferably, the compatibilizer is a maleic anhydride grafted compatibilizer.
Preferably, the antioxidant consists of an antioxidant 168, an antioxidant 1076 and an antioxidant CA according to the mass ratio of 1:0.5-0.6:0.12-0.18.
Preferably, in the fourth step, the film blowing master batch is put into a film blowing machine, the temperature of a screw is 140-165 ℃, the processing temperature of a die head is 165-175 ℃, and the film blowing thickness is 8-12 mu m.
As can be seen from the above description of the present invention, compared with the prior art, the present invention has the following beneficial effects: the invention uses PBAT and polylactic acid as the base materials to be matched with the added modified attapulgite, styrene-maleic anhydride copolymer and other auxiliary agents to obtain the degradable mulch film with good light weight and toughness, thereby improving the tearing strength of the degradable mulch film; wherein, the styrene-maleic anhydride copolymer is matched with the modified attapulgite to effectively improve the toughness of the prepared mulching film, further improve the tearing strength of the degradable mulching film and meet the production requirement; the addition of the modified attapulgite with a porous structure can also reduce the addition of other chemical additives, reduce the production cost and obviously reduce the weight of the mulching film; meanwhile, the prepared mulching film can adapt to the change of air temperature, so that the temperature which rises suddenly and falls suddenly is prevented from influencing the mulching film favorably, the service life of the mulching film is prolonged, and the maintenance cost is reduced;
the modification step of the modified attapulgite is limited, so that the surface stress of the modified attapulgite is reduced, agglomeration is prevented, uniform dispersion of the modified attapulgite is facilitated, and the modified attapulgite is effectively matched with other auxiliary agents, so that the mechanical properties of the prepared degradable mulching film are improved, and the production requirement is met;
the composition of the light stabilizer and the antioxidant is specifically limited, and the light stabilizer and the antioxidant are matched with each other, so that the possibility of photochemical reaction can be eliminated or slowed down under the irradiation of light, and the photo-aging process is prevented or delayed, thereby achieving the purpose of prolonging the service life of the degradable mulch film.
Detailed Description
The invention is further described below by means of specific embodiments.
The PBAT degradable mulch film consists of the following raw materials in parts by weight: 50-70 parts of PBAT, 0.8-2 parts of epoxidized soybean oil, 0.7-1.5 parts of antioxidant, 25-35 parts of polylactic acid, 10-15 parts of modified attapulgite, 0.1-0.5 part of acetyl triethyl citrate, 3-5 parts of styrene-maleic anhydride copolymer, 1-2 parts of maleic anhydride grafting compatilizer and 0.5-0.8 part of lubricant.
Wherein the lubricant is polyethylene wax or oleamide.
The antioxidant consists of antioxidant 168, antioxidant 1076 and antioxidant CA in the mass ratio of 1 to 0.5-0.6 to 0.12-0.18.
The preparation method comprises the following steps:
step one, weighing and mixing PBAT, polylactic acid and modified attapulgite according to the required weight parts, and then heating and baking at 80-100 ℃ until the water content is lower than 0.5%;
step two, weighing other raw materials according to the required weight parts, and then sending the mixture obtained in the step one into a high-speed mixer, and uniformly mixing to obtain a premix;
step three, putting the premix obtained in the step two into a double-screw extruder, and controlling the extrusion temperature between 150 and 180 ℃ to obtain film blowing master batch;
and fourthly, blowing the film blowing master batch into a film by a film blowing machine, controlling the temperature of a screw to be 140-165 ℃, the processing temperature of a die head to be 165-175 ℃ and the film blowing thickness to be 8-12 mu m, and obtaining the PBAT degradable mulch film.
The preparation method of the modified attapulgite comprises the following steps:
(1) Crushing attapulgite to 10-20 meshes, adding the crushed attapulgite into water, uniformly stirring, soaking for more than 12 hours, centrifuging, filtering, and drying for later use;
(2) Adding the attapulgite treated in the step (1) into a phosphoric acid solution with the mass concentration of 5%, stirring and heating, wherein the stirring speed is 180-250r/min, and the heating temperature is 80-90 ℃; then filtering to remove phosphoric acid solution, washing attapulgite with weak base solution to neutrality, washing with deionized water for 2-3 times, and drying for standby;
(3) Raising the temperature of the attapulgite obtained in the step (2) to 250-300 ℃ from room temperature, enabling water vapor to contact and react with the attapulgite through inert gas, starting to cool after the reaction is finished, and stopping adding the water vapor; and after the temperature is reduced to room temperature, taking out the attapulgite, washing and drying until the water content is lower than 5%, and grinding and crushing to obtain the nano-grade modified attapulgite.
Example 1
The PBAT degradable mulch film consists of the following raw materials in parts by weight: 50 parts of PBAT, 0.8 part of epoxidized soybean oil, 1.5 parts of antioxidant, 35 parts of polylactic acid, 10 parts of modified attapulgite, 0.5 part of acetyl triethyl citrate, 3 parts of styrene-maleic anhydride copolymer, 2 parts of maleic anhydride grafting compatilizer and 0.5 part of polyethylene wax.
The antioxidant consists of an antioxidant 168, an antioxidant 1076 and an antioxidant CA according to the mass ratio of 1:0.5:0.12.
The preparation method comprises the following steps:
step one, weighing and mixing PBAT, polylactic acid and modified attapulgite according to the required weight parts, and then heating at 80 ℃ until the water content is lower than 0.5%;
step two, weighing other raw materials according to the required weight parts, and then sending the mixture obtained in the step one into a high-speed mixer, and uniformly mixing to obtain a premix;
step three, putting the premix obtained in the step two into a double-screw extruder, and controlling the extrusion temperature at 150 ℃ to obtain film blowing master batch;
and fourthly, blowing the film blowing master batch into a film by a film blowing machine, controlling the temperature of a screw to 140 ℃, the processing temperature of a die head to 165 ℃, and blowing the film to a thickness of 12 mu m to obtain the PBAT degradable mulch film.
The preparation method of the modified attapulgite comprises the following steps:
(1) Crushing attapulgite to 10-20 meshes, adding the crushed attapulgite into water, uniformly stirring, soaking for more than 12 hours, centrifuging, filtering, and drying for later use;
(2) Adding the attapulgite treated in the step (1) into a phosphoric acid solution with the mass concentration of 5%, stirring and heating, wherein the stirring speed is 180r/min, and the heating temperature is 80 ℃; then filtering to remove phosphoric acid solution, washing attapulgite with weak base solution to be neutral, washing with deionized water for 2 times, and drying for later use;
(3) Raising the temperature of the attapulgite obtained in the step (2) from room temperature to 250 ℃, enabling water vapor to contact and react with the attapulgite through inert gas, starting to cool after the reaction is finished, and stopping adding the water vapor; and after the temperature is reduced to room temperature, taking out the attapulgite, washing and drying until the water content is lower than 5%, and grinding and crushing to obtain the nano-grade modified attapulgite.
Example 2
The PBAT degradable mulch film consists of the following raw materials in parts by weight: 70 parts of PBAT, 2 parts of epoxidized soybean oil, 0.7 part of antioxidant, 25 parts of polylactic acid, 15 parts of modified attapulgite, 0.1 part of acetyl triethyl citrate, 5 parts of styrene-maleic anhydride copolymer, 1 part of maleic anhydride grafting compatilizer and 0.8 part of oleamide.
The antioxidant consists of an antioxidant 168, an antioxidant 1076 and an antioxidant CA according to the mass ratio of 1:0.6:0.18.
The preparation method comprises the following steps:
step one, weighing and mixing PBAT, polylactic acid and modified attapulgite according to the required weight parts, and then heating at 100 ℃ until the water content is lower than 0.5%;
step two, weighing other raw materials according to the required weight parts, and then sending the mixture obtained in the step one into a high-speed mixer, and uniformly mixing to obtain a premix;
step three, putting the premix obtained in the step two into a double-screw extruder, and controlling the extrusion temperature at 180 ℃ to obtain film blowing master batch;
and fourthly, blowing the film blowing master batch into a film by a film blowing machine, controlling the temperature of a screw rod to 165 ℃, the processing temperature of a die head to 175 ℃, and blowing the film to a thickness of 8 mu m to obtain the PBAT degradable mulch film.
The preparation method of the modified attapulgite comprises the following steps:
(1) Crushing attapulgite to 10-20 meshes, adding the crushed attapulgite into water, uniformly stirring, soaking for more than 12 hours, centrifuging, filtering, and drying for later use;
(2) Adding the attapulgite treated in the step (1) into a phosphoric acid solution with the mass concentration of 5%, stirring and heating, wherein the stirring speed is 250r/min, and the heating temperature is 90 ℃; then filtering to remove phosphoric acid solution, washing attapulgite with weak base solution to be neutral, washing with deionized water for 3 times, and drying for later use;
(3) Raising the temperature of the attapulgite obtained in the step (2) from room temperature to 300 ℃, enabling water vapor to contact and react with the attapulgite through inert gas, starting to cool after the reaction is finished, and stopping adding the water vapor; and after the temperature is reduced to room temperature, taking out the attapulgite, washing and drying until the water content is lower than 5%, and grinding and crushing to obtain the nano-grade modified attapulgite.
Example 3
The PBAT degradable mulch film consists of the following raw materials in parts by weight: 60 parts of PBAT, 1.5 parts of epoxidized soybean oil, 1.2 parts of antioxidant, 30 parts of polylactic acid, 12 parts of modified attapulgite, 0.3 part of acetyl triethyl citrate, 4 parts of styrene-maleic anhydride copolymer, 1.5 parts of maleic anhydride grafting compatilizer and 0.65 part of polyethylene wax.
The antioxidant consists of an antioxidant 168, an antioxidant 1076 and an antioxidant CA according to the mass ratio of 1:0.55:0.15.
The preparation method comprises the following steps:
step one, weighing and mixing PBAT, polylactic acid and modified attapulgite according to the required weight parts, and then heating and baking at 90 ℃ until the water content is lower than 0.5%;
step two, weighing other raw materials according to the required weight parts, and then sending the mixture obtained in the step one into a high-speed mixer, and uniformly mixing to obtain a premix;
step three, putting the premix obtained in the step two into a double-screw extruder, and controlling the extrusion temperature to 170 ℃ to obtain film blowing master batch;
and fourthly, blowing the film blowing master batch into a film by a film blowing machine, controlling the temperature of a screw to 160 ℃, the processing temperature of a die head to 170 ℃, and blowing the film to a thickness of 10 mu m to obtain the PBAT degradable mulch film.
The preparation method of the modified attapulgite comprises the following steps:
(1) Crushing attapulgite to 10-20 meshes, adding the crushed attapulgite into water, uniformly stirring, soaking for more than 12 hours, centrifuging, filtering, and drying for later use;
(2) Adding the attapulgite treated in the step (1) into a phosphoric acid solution with the mass concentration of 5%, stirring and heating, wherein the stirring speed is 220r/min, and the heating temperature is 85 ℃; then filtering to remove phosphoric acid solution, washing attapulgite with weak base solution to neutrality, washing with deionized water for 2-3 times, and drying for standby;
(3) Raising the temperature of the attapulgite obtained in the step (2) to 275 ℃ from room temperature, enabling water vapor to contact and react with the attapulgite through inert gas, starting to cool after the reaction is finished, and stopping adding the water vapor; and after the temperature is reduced to room temperature, taking out the attapulgite, washing and drying until the water content is lower than 5%, and grinding and crushing to obtain the nano-grade modified attapulgite.
Comparative example 1
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: the raw material composition is not added with modified attapulgite.
Comparative example 2
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: the styrene-maleic anhydride copolymer is not added in the raw material composition.
Contrast Liu 3
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: the raw material composition is not added with modified attapulgite and styrene-maleic anhydride copolymer.
Comparative example 4
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: the attapulgite added in the raw material composition is common attapulgite, and no modification treatment is performed.
Comparative example 5
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: the epoxidized soybean oil is not added in the raw material composition.
Comparative example 6
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: in the antioxidant composition, antioxidant 168 is replaced by antioxidant 1010.
Comparative example 7
The raw material composition and the preparation method are basically the same as those of the example 3, and the difference is that: in the composition of the antioxidant, the antioxidant consists of an antioxidant 168 and an antioxidant CA according to the mass ratio of 1:0.15.
The mulching films prepared in examples 1 to 3 and comparative examples 1 to 7 were subjected to corresponding tests to obtain the following data:
table 1 test data sheet for various embodiments
As can be seen from the table, the invention is characterized in that the raw material composition of the degradable mulch film is limited, and the degradable mulch film is prepared by taking PBAT and polylactic acid as the bases and adding modified attapulgite, styrene-maleic anhydride copolymer and other auxiliary agents, so that the degradable mulch film with good light weight and toughness is obtained, and the tearing strength of the degradable mulch film is improved.
As can be seen from the comparison of the example 3 and the comparative examples 1-3, the addition of the styrene-maleic anhydride copolymer and the modified attapulgite can effectively improve the toughness of the prepared mulching film, further improve the tearing strength of the degradable mulching film and meet the production requirements; the addition of the modified attapulgite with a porous structure can also reduce the addition of other chemical additives, reduce the production cost and obviously reduce the weight of the mulching film; meanwhile, the prepared mulching film can adapt to the change of air temperature, and the temperature suddenly rising and suddenly falling is prevented from influencing the mulching film favorably, so that the service life of the mulching film is prolonged, and the maintenance cost is reduced.
As can be seen by comparing the embodiment 3 with the comparative example 4, the modification step of the modified attapulgite is limited, the surface stress of the modified attapulgite is reduced, agglomeration is prevented, the modified attapulgite is uniformly dispersed and is effectively matched with other auxiliary agents, the mechanical property of the prepared degradable mulch film is further improved, and the production requirement is met;
as can be seen from the comparison of the example 3 and the comparative examples 5 to 7, the compositions of the light stabilizer and the antioxidant are specifically limited, and the combination of the light stabilizer and the antioxidant can eliminate or slow down the possibility of photochemical reaction under the irradiation of light, and prevent or delay the photo-aging process, thereby achieving the purpose of prolonging the service life of the degradable mulch film.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, i.e., the invention is not to be limited to the details of the claims and the description, but rather is to cover all modifications which are within the scope of the invention.
Claims (5)
1. A preparation method of a PBAT degradable mulch film is characterized by comprising the following steps: the PBAT degradable mulch film comprises the following raw materials in parts by weight: 50-70 parts of PBAT, 0.8-2 parts of epoxidized soybean oil, 0.7-1.5 parts of antioxidant, 25-35 parts of polylactic acid, 10-15 parts of modified attapulgite, 0.1-0.5 part of acetyl triethyl citrate, 3-5 parts of styrene-maleic anhydride copolymer, 1-2 parts of compatilizer and 0.5-0.8 part of lubricant;
the preparation method comprises the following steps:
step one, weighing and mixing PBAT, polylactic acid and modified attapulgite according to the required weight parts, and then heating and baking at 80-100 ℃ until the water content is lower than 0.5%;
step two, weighing other raw materials according to the required weight parts, and then sending the mixture obtained in the step one into a high-speed mixer, and uniformly mixing to obtain a premix;
step three, putting the premix obtained in the step two into a double-screw extruder, and controlling the extrusion temperature between 150 and 180 ℃ to obtain film blowing master batch;
blowing the film blowing master batch into a film by a film blowing machine to obtain the PBAT degradable mulch film;
the preparation method of the modified attapulgite comprises the following steps:
(1) Crushing attapulgite to 10-20 meshes, adding the crushed attapulgite into water, uniformly stirring, soaking for more than 12 hours, centrifuging, filtering, and drying for later use;
(2) Adding the attapulgite treated in the step (1) into a phosphoric acid solution, stirring and heating, wherein the stirring speed is 180-250r/min, and the heating temperature is 80-90 ℃; then filtering to remove phosphoric acid solution, washing attapulgite with weak base solution to neutrality, washing with deionized water for 2-3 times, and drying for standby;
(3) Raising the temperature of the attapulgite obtained in the step (2) to 250-300 ℃ from room temperature, enabling water vapor to contact and react with the attapulgite through inert gas, starting to cool after the reaction is finished, and stopping adding the water vapor; after the temperature is reduced to room temperature, the attapulgite is taken out, washed and dried until the water content is lower than 5%, and ground and crushed to obtain nano-grade modified attapulgite;
the antioxidant consists of an antioxidant 168, an antioxidant 1076 and an antioxidant CA according to the mass ratio of 1:0.5-0.6:0.12-0.18.
2. The method for preparing the PBAT degradable mulch film according to claim 1, which is characterized in that: in the step (2), the mass concentration of the phosphoric acid solution is 5%.
3. The method for preparing the PBAT degradable mulch film according to claim 1, which is characterized in that: the lubricant is polyethylene wax or oleamide.
4. The method for preparing the PBAT degradable mulch film according to claim 1, which is characterized in that: the compatilizer is a maleic anhydride grafting compatilizer.
5. The method for preparing the PBAT degradable mulch film according to claim 1, which is characterized in that: in the fourth step, the film blowing master batch is put into a film blowing machine, the temperature of a screw is 140-165 ℃, the processing temperature of a die head is 165-175 ℃, and the film blowing thickness is 8-12 mu m.
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